CN103951806A - Low molecular weight phenolic resin impregnation liquid for manufacturing sticky membrane paper and preparation method of low molecular weight phenolic resin impregnation liquid - Google Patents
Low molecular weight phenolic resin impregnation liquid for manufacturing sticky membrane paper and preparation method of low molecular weight phenolic resin impregnation liquid Download PDFInfo
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- CN103951806A CN103951806A CN201410199928.7A CN201410199928A CN103951806A CN 103951806 A CN103951806 A CN 103951806A CN 201410199928 A CN201410199928 A CN 201410199928A CN 103951806 A CN103951806 A CN 103951806A
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Abstract
The invention relates to the field of polymer materials and provides a low molecular weight phenolic resin impregnation liquid for manufacturing sticky membrane paper and a preparation method of the low molecular weight phenolic resin impregnation liquid. Phenol and formaldehyde are used as main raw materials, sodium hydroxide is used as a catalyst, and a wear-resistant agent, a dispersing agent and a solvent are added in a resin synthesis process, so that a uniform composite system is formed. Formaldehyde and water are added twice in the concrete preparation process, so that the reaction process is stable, and the reaction product is uniform; initial resin with low polymerization degree, uniform molecular weight and low viscosity is obtained through controlling the condensation polymerization temperature and the reaction endpoint; the wear-resistant agent, the dispersing agent and the solvent are added in the resin, so that the wear resistance and toughness of the cured resin are improved, and furthermore, the wear resistance and toughness of the sticky membrane paper are improved.
Description
Technical field
The present invention relates to polymeric material field, specifically refer to a kind of for improving pf resin of low molecular weight steeping fluid of manufacturing for bond paper of impregnated bond paper wear resistance and preparation method thereof.
Background technology
Bond paper is a kind of surface decoration material for timber and wood-based plate, and it both can be used alone, and also can be pressed into decorative laminate with thin material composite gum such as multilayer laminate paper or veneers.Bond paper and decorative laminate can be widely used in the fields such as various table tops, floor, furniture, vehicle, aircraft, boats and ships, decontamination chamber, instrument, household electrical appliance, building interior trim.Bond paper is with synthetic resins, various special paper to be flooded, and makes resin infiltrate paper inside, be filled in the space of paper inside, then a kind of gum dipped paper of obtaining of drying processing.According to condition differences such as paper color, decorative pattern, pattern, thickness, bond paper has colourful outward appearance and different physical and mechanical properties.One or more layers bond paper is pasted on surface at timber (being mainly some low grades, low-grade wood) and wood-based plate (being mainly fiberboard, shaving board etc.), not only can beautify the surface of timber and wood-based plate, and can improve surface hardness, wear resistance, smooth finish and other physical and mechanical property of timber and wood-based plate, and can play sealing wood-based plate surface, prevent the effect that in plate, formaldehyde discharges.
Resol is a kind of artificial synthetic resin, in producing, bond paper is widely applied, but common resol is as dipping resin, there is following several respects problem: 1, higher due to molecular resin polycondensation, crosslinking degree, molecular resin amount is larger, and perviousness is poor, make it in the time producing bond paper, being difficult for infiltrating paper inside, easily there is starved, few glue phenomenon in the sandwich layer of bond paper, causes the quality of bond paper to reduce.2, because molecular resin amount is large, perviousness is poor, and in bond paper is produced, processing parameter regulation and control are more difficult, has increased the difficulty of operation.Although 3, common resol also has certain wear resistance after solidifying, for the surface decoration that has high-wearing feature to require, its wear resistance is just difficult to satisfy the demand.4, after common phenolic resin curing, fragility is larger, and under the environmental influences such as air, illumination, temperature, humidity, crack performance easily occurs on surface, thereby has influence on the surface decoration quality of product.
Summary of the invention
The deficiency existing for prior art, the object of the invention is to prepare compared with the resol using in a kind of and current production, molecular weight is low, good penetrability, solidify after the bond paper of good toughness, production there is the resin impregnating liquid of high-wearing feature.In this resin impregnating liquid, contain anti-wear agent and dispersion agent, anti-wear agent, dispersion agent and uniform compound system of resin formation, the bond paper that the bond paper of producing with this composite phenolic resin steeping fluid is produced than common resol has better wear resistance and toughness, can be widely used in the surface decoration of timber, wood-based plate.
For realizing above object, the technical solution used in the present invention is:
A pf resin of low molecular weight steeping fluid of manufacturing for bond paper, is grouped into by the one-tenth of following weight part:
100 parts of phenol
100 parts-125 parts of formalins
10 parts-25 parts of alkaline catalystss
60 parts-70 parts, water
0.5 part-1.5 parts of anti-wear agents
0.4 part-12 parts of dispersion agents
12 parts-25 parts of alcoholic solvents;
Wherein, described anti-wear agent is selected from one or both in silicon carbide, silicon-dioxide; Described dispersion agent is selected from one or more in Microcrystalline Cellulose, sodium alginate and carboxymethyl cellulose.
Preferred version: the one-tenth by following weight part is grouped into:
100 parts of phenol
105 parts-120 parts of formalins
11 parts-17 parts of alkaline catalystss
61 parts-68 parts, water
0.6 part-1.2 parts of anti-wear agents
0.4 part-12 parts of dispersion agents
15 parts-17 parts of alcoholic solvents.
The massfraction of described formalin is preferably 30%-40%.
Described alkaline catalysts is the aqueous sodium hydroxide solution that massfraction is preferably 20%-40%.
Described alcoholic solvent is preferably the ethanol of massfraction >=75%.
Described dispersion agent is preferably one of following three kinds of schemes:
Scheme one: described dispersion agent is Microcrystalline Cellulose and sodium alginate, wherein Microcrystalline Cellulose is the 6.8%-10.5% of phenol quality, sodium alginate is the 0.14%-0.28% of phenol quality;
Scheme two: described dispersion agent is carboxymethyl cellulose, wherein carboxymethyl cellulose is the 0.4%-0.5% of phenol quality;
Scheme three: described dispersion agent is preferably Microcrystalline Cellulose, sodium alginate and carboxymethyl cellulose, wherein Microcrystalline Cellulose is the 6.8%-10.5% of phenol quality, sodium alginate is the 0.14%-0.28% of phenol quality, and carboxymethyl cellulose is the 0.4%-0.5% of phenol quality.
The preparation method of the described pf resin of low molecular weight steeping fluid of manufacturing for bond paper, concrete grammar is:
According to said ratio, phenol, alkaline catalysts and first water are mixed, at 45 DEG C-55 DEG C following 10-15min that keep, then add first formaldehyde, be slowly warming up to 88 DEG C-90 DEG C, keep being cooled to 80 DEG C-85 DEG C after 10-15min, add residual formaldehyde, be warming up to again 88 DEG C-90 DEG C, and at this temperature reaction to terminal, recording at 20 DEG C when viscosity is 40-45mPaS is reaction end; Reach after reaction end and add remaining water, then cooling down, while being cooled to 70 DEG C-80 DEG C, adds anti-wear agent and dispersion agent, then under whipped state, is cooled to 40 DEG C-45 DEG C time and adds alcoholic solvent, continues to be cooled to 35 DEG C of following blowings; Described first water accounts for the 30%-40% of water total mass, and first formaldehyde accounts for the 70%-80% of formaldehyde total mass.
Explanation that the present invention will be further explained below:
The present invention is in concrete preparation process, and formaldehyde divides secondary to add to have improved the stationarity of phenol and formaldehyde reaction, and impels phenol more complete with reacting of formaldehyde, makes free-phenol and free formaldehyde content in resin lower.Polycondensation temperature is controlled to 88-90 DEG C (common resol is 94-96 DEG C), can makes the unlikely too fierceness of polycondensation of the adduct-hydroxymethyl phenol of phenol and formaldehyde, thereby improve the polymerization homogeneity of molecular resin.The synthetic control of reaction end point of resin is at 40-45mPaS(20 DEG C), can control the polymerization degree of molecular resin, form low-molecular-weight resin, make resin there is good perviousness, in the time producing bond paper, paper can be soaked into completely.Second batch water add the temperature that can reduce rapidly resin, and resin is diluted, the polycondensation of resin is stopped, keeping the lower molecular weight state of resin.Adding of anti-wear agent, can improve the wear resistance of bond paper, anti-wear agent can resin be carrier, enters paper inside together with resin.The effect of dispersion agent is that anti-wear agent is dispersed in resin, and unlikely anti-wear agent forms precipitation.Solvent add the perviousness that can improve resin, and can reduce the fragility after resin solidification, increase the toughness of bond paper.
Of the present invention a kind of as follows for improving the technical indicator of pf resin of low molecular weight steeping fluid of bond paper wear resistance:
Solids content 40%-45%; Terminal viscosity 40-45mPas; Free phenol content < 1.0%, content of free aldehyde < 0.3%; PH value 8.5-9.2; Molecular-weight average 250-350; 3 times of water Combination >; Steady time > 45 days.
Compared with prior art, advantage of the present invention is:
1, low, the good penetrability of steeping fluid molecular weight of the present invention, good stability, after solidifying, the bond paper of good toughness, production has high-wearing feature.
2, steeping fluid of the present invention has good perviousness and solidifies rear toughness, with can reach≤0.06g/100r(of the wear resistance national standard of the bond paper decorative laminate of this production of resins be≤0.08g/100r), improve the service efficiency of impregnated bond paper and the surface quality of veneer product, can meet the requirement of the bond paper veneer product with high-wearing feature requirement.
Embodiment
Below the present invention is further explained and is illustrated, phenol described in embodiment is more than 98% Phenol,Solid of purity; Described formaldehyde is that massfraction is 37% formalin; Described alkaline catalysts is that massfraction is 30% aqueous sodium hydroxide solution; Described solvent is that massfraction is 75% industrial alcohol.
embodiment 1
Take respectively phenol 500kg, sodium hydroxide solution 55kg, first formaldehyde solution 394kg, the
Two crowdes of formaldehyde solution 131kg, first water 107kg, second batch water 198kg, silicon carbide 3kg, sea
Sodiun alginate 0.75kg, Microcrystalline Cellulose 34kg, ethanol 85kg.
Phenol, 55kg sodium hydroxide solution and the 107kg water of 500kg fusing are added to reactor, start agitator, at 50 DEG C of following 10-15min that keep, add first formaldehyde solution 394kg, be slowly warming up to 88-90 DEG C, keep being cooled to 82 DEG C of left and right after 15-20min, add second batch formaldehyde solution 131kg, be warming up to again 88-90 DEG C, and react (20 DEG C, 40-45mPaS is reaction end) to terminal at this temperature.Add second batch water 198kg, and cooling down, while being cooled to 70-80 DEG C, add silicon carbide 3kg, sodium alginate 0.75kg and Microcrystalline Cellulose 34kg, stir while being cooled to 45 DEG C of left and right, adds ethanol 85kg, continues to be cooled to 35 DEG C of blowings when following.
The quality index of resin: solids content 43.8 %; Terminal viscosity 45mPas; Free phenol content 0.95%, free formaldehyde content 0.21%; PH value 8.6; Molecular-weight average 250-350; 3 times of water Combination >; Steady time > 45 days.
Can reach≤0.06g/100r(of the wear resistance national standard of the bond paper decorative laminate of producing with this resin impregnation liquid is≤0.08g/100r), improve the wear resistance of bond paper.
embodiment 2
Take respectively phenol 500kg, sodium hydroxide solution 70kg, first formaldehyde solution 431kg, second batch formaldehyde solution 144kg, first water 112kg, second batch water 208kg, silicon-dioxide 4.5kg, sodium alginate 1.05kg, Microcrystalline Cellulose 42.5kg, ethanol 90kg.
Phenol, 70kg sodium hydroxide solution and the 112kg water of 500kg fusing are added to reactor, start agitator, at 50 DEG C of following 10-15min that keep, add first formaldehyde solution 431kg, be slowly warming up to 88-90 DEG C, keep being cooled to 82 DEG C of left and right after 15-20min, add second batch formaldehyde solution 144kg, be warming up to again 88-90 DEG C, and react (20 DEG C, 40-45mPaS is reaction end) to terminal at this temperature.Add second batch water 208kg, and cooling down, while being cooled to 70-80 DEG C, add silicon-dioxide 4.5kg, sodium alginate 1.05kg and Microcrystalline Cellulose 42.5kg, stir while being cooled to 45 DEG C of left and right, adds ethanol 90kg, continues to be cooled to 35 DEG C of blowings when following.
The quality index of resin: solids content 43.2%; Terminal viscosity 43mPas; Free phenol content 0.87%, free formaldehyde content 0.25%; PH value 8.7; Molecular-weight average 250-350; 3 times of water Combination >; Steady time > 45 days.
Can reach≤0.06g/100r(of the wear resistance national standard of the bond paper decorative laminate of producing with this resin impregnation liquid is≤0.08g/100r), improve the wear resistance of bond paper.
embodiment 3
Take respectively phenol 500kg, sodium hydroxide solution 85kg, first formaldehyde solution 469kg, second batch formaldehyde solution 156kg, first water 120kg, second batch water 220kg, silicon-dioxide 2.5kg, silicon carbide 3.5kg, carboxymethyl cellulose 3.8kg, alcohol 95 kg.
Phenol, 85kg sodium hydroxide solution and the 120kg water of 500kg fusing are added to reactor, start agitator, at 50 DEG C of following 10-15min that keep, add first formaldehyde solution 469kg, be slowly warming up to 88-90 DEG C, keep being cooled to 82 DEG C of left and right after 15-20min, add second batch formaldehyde solution 156kg, be warming up to again 88-90 DEG C, and react (20 DEG C, 40-45mPaS is reaction end) to terminal at this temperature.Add second batch water 220kg, and cooling down, while being cooled to 70-80 DEG C, add silicon-dioxide 2.5kg, silicon carbide 3.5kg and carboxymethyl cellulose 3.8kg, stir while being cooled to 45 DEG C of left and right, adds alcohol 95 kg, continues to be cooled to 35 DEG C of blowings when following.
The quality index of resin: solids content 42.7%; Terminal viscosity 42mPas; Free phenol content 0.76%, free formaldehyde content 0.27%; PH value 9.1; Molecular-weight average 250-350; 3 times of water Combination >; Steady time > 45 days.
Can reach≤0.06g/100r(of the wear resistance national standard of the bond paper decorative laminate of producing with this resin impregnation liquid is≤0.08g/100r), improve the wear resistance of bond paper.
embodiment 4
Take respectively phenol 500kg, sodium hydroxide solution 85kg, first formaldehyde solution 470kg, second batch formaldehyde solution 156kg, first water 120kg, second batch water 220kg, silicon-dioxide 2.5kg, silicon carbide 3.5kg, sodium alginate 1.05kg, Microcrystalline Cellulose 42.5kg, carboxymethyl cellulose 3.8kg, alcohol 95 kg.
Phenol, 85kg sodium hydroxide solution and the 120kg water of 500kg fusing are added to reactor, start agitator, at 50 DEG C of following 10-15min that keep, add first formaldehyde solution 469kg, be slowly warming up to 88-90 DEG C, keep being cooled to 82 DEG C of left and right after 15-20min, add second batch formaldehyde solution 156kg, be warming up to again 88-90 DEG C, and react (20 DEG C, 40-45mPaS is reaction end) to terminal at this temperature.Add second batch water 220kg, and cooling down, while being cooled to 70-80 DEG C, add silicon-dioxide 2.5kg, silicon carbide 3.5kg and carboxymethyl cellulose 3.8kg, stir while being cooled to 45 DEG C of left and right, adds alcohol 95 kg, continues to be cooled to 35 DEG C of blowings when following.
The quality index of resin: solids content 42.5%; Terminal viscosity 41mPas; Free phenol content 0.6%, free formaldehyde content 0.25%; PH value 9.0; Molecular-weight average 250-350; 3 times of water Combination >; Steady time > 45 days.
With can reach≤0.06g/100r(of the wear resistance national standard of the bond paper decorative laminate of this production of resins be≤0.08g/100r), improved the wear resistance of bond paper.
Claims (7)
1. a pf resin of low molecular weight steeping fluid of manufacturing for bond paper, is characterized in that, is grouped into by the one-tenth of following weight part:
100 parts of phenol
100 parts-125 parts of formalins
10 parts-25 parts of alkaline catalystss
60 parts-70 parts, water
0.5 part-1.5 parts of anti-wear agents
0.4 part-12 parts of dispersion agents
12 parts-25 parts of alcoholic solvents;
Wherein, described anti-wear agent is selected from one or both in silicon carbide, silicon-dioxide; Described dispersion agent is selected from one or more in Microcrystalline Cellulose, sodium alginate and carboxymethyl cellulose.
2. the pf resin of low molecular weight steeping fluid of manufacturing for bond paper according to claim 1, is characterized in that, is grouped into by the one-tenth of following weight part:
100 parts of phenol
105 parts-120 parts of formalins
11 parts-17 parts of alkaline catalystss
61 parts-68 parts, water
0.6 part-1.2 parts of anti-wear agents
0.4 part-12 parts of dispersion agents
15 parts-17 parts of alcoholic solvents.
3. the pf resin of low molecular weight steeping fluid of manufacturing for bond paper according to claim 1, is characterized in that, the massfraction of described formalin is 30%-40%.
4. the pf resin of low molecular weight steeping fluid of manufacturing for bond paper according to claim 1, is characterized in that, described alkaline catalysts is that massfraction is the aqueous sodium hydroxide solution of 20%-40%.
5. the pf resin of low molecular weight steeping fluid of manufacturing for bond paper according to claim 1, is characterized in that the ethanol that described alcoholic solvent is massfraction >=75%.
6. according to the pf resin of low molecular weight steeping fluid of manufacturing for bond paper one of claim 1-5 Suo Shu, it is characterized in that, described dispersion agent is one of following three kinds of schemes:
Scheme one: described dispersion agent is Microcrystalline Cellulose and sodium alginate, wherein Microcrystalline Cellulose is the 6.8%-10.5% of phenol quality, sodium alginate is the 0.14%-0.28% of phenol quality;
Scheme two: described dispersion agent is carboxymethyl cellulose, wherein carboxymethyl cellulose is the 0.4%-0.5% of phenol quality;
Scheme three: described dispersion agent is preferably Microcrystalline Cellulose, sodium alginate and carboxymethyl cellulose, wherein Microcrystalline Cellulose is the 6.8%-10.5% of phenol quality, sodium alginate is the 0.14%-0.28% of phenol quality, and carboxymethyl cellulose is the 0.4%-0.5% of phenol quality.
7. the preparation method of the described pf resin of low molecular weight steeping fluid of manufacturing for bond paper of one of claim 1-6, is characterized in that, concrete grammar is:
According to said ratio, phenol, alkaline catalysts and first water are mixed, at 45 DEG C-55 DEG C following 10-15min that keep, then add first formaldehyde, be slowly warming up to 88 DEG C-90 DEG C, keep being cooled to 80 DEG C-85 DEG C after 10-15min, add residual formaldehyde, be warming up to again 88 DEG C-90 DEG C, and at this temperature reaction to terminal, recording at 20 DEG C when viscosity is 40-45mPaS is reaction end; Reach after reaction end and add remaining water, then cooling down, while being cooled to 70 DEG C-80 DEG C, adds anti-wear agent and dispersion agent, then under whipped state, is cooled to 40 DEG C-45 DEG C time and adds alcoholic solvent, continues to be cooled to 35 DEG C of following blowings; Described first water accounts for the 30%-40% of water total mass, and first formaldehyde accounts for the 70%-80% of formaldehyde total mass.
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| CN201410199928.7A CN103951806B (en) | 2014-05-13 | 2014-05-13 | A kind of pf resin of low molecular weight steeping fluid for bond paper manufacture and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877097A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Preparation method of phenol formaldehyde resin |
| CN107283552A (en) * | 2017-08-15 | 2017-10-24 | 周健雄 | One kind makes plywood method |
| CN109679044A (en) * | 2018-12-21 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003956A (en) * | 2007-01-12 | 2007-07-25 | 东华大学 | Composite conductive paper of carbon fiber |
| JP2011084703A (en) * | 2009-10-15 | 2011-04-28 | Chan Sieh Enterprises Co Ltd | Cured globular particle of phenol resin containing bubble, and manufacturing method thereof |
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2014
- 2014-05-13 CN CN201410199928.7A patent/CN103951806B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003956A (en) * | 2007-01-12 | 2007-07-25 | 东华大学 | Composite conductive paper of carbon fiber |
| JP2011084703A (en) * | 2009-10-15 | 2011-04-28 | Chan Sieh Enterprises Co Ltd | Cured globular particle of phenol resin containing bubble, and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 盛菊华: "合成树脂装饰板的阻燃处理及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877097A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Preparation method of phenol formaldehyde resin |
| CN107283552A (en) * | 2017-08-15 | 2017-10-24 | 周健雄 | One kind makes plywood method |
| CN109679044A (en) * | 2018-12-21 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper |
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